US7764379B1 - Semiconductor laser natural gas analysis system and method - Google Patents

Semiconductor laser natural gas analysis system and method Download PDF

Info

Publication number
US7764379B1
US7764379B1 US11/613,291 US61329106A US7764379B1 US 7764379 B1 US7764379 B1 US 7764379B1 US 61329106 A US61329106 A US 61329106A US 7764379 B1 US7764379 B1 US 7764379B1
Authority
US
United States
Prior art keywords
gas
interest
tunable
energy content
pressure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
US11/613,291
Inventor
Lawrence McDermott
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Excelitas Technologies Corp
Original Assignee
Axsun Technologies LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Axsun Technologies LLC filed Critical Axsun Technologies LLC
Priority to US11/613,291 priority Critical patent/US7764379B1/en
Assigned to AXSUN TECHNOLOGIES, INC. reassignment AXSUN TECHNOLOGIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MCDERMOTT, LAWRENCE
Application granted granted Critical
Publication of US7764379B1 publication Critical patent/US7764379B1/en
Assigned to AXSUN TECHNOLOGIES LLC reassignment AXSUN TECHNOLOGIES LLC CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: AXSUN TECHNOLOGIES, INC.
Assigned to AXSUN TECHNOLOGIES, INC. reassignment AXSUN TECHNOLOGIES, INC. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: Axsun Technologies, LLC
Assigned to JPMORGAN CHASE BANK, N.A. reassignment JPMORGAN CHASE BANK, N.A. FIRST LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT Assignors: AXSUN TECHNOLOGIES, INC.
Assigned to ROYAL BANK OF CANADA, AS COLLATERAL AGENT reassignment ROYAL BANK OF CANADA, AS COLLATERAL AGENT SECOND LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT Assignors: AXSUN TECHNOLOGIES, INC.
Assigned to Excelitas Technologies Corp. reassignment Excelitas Technologies Corp. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AXSUN TECHNOLOGIES INC.
Assigned to AXSUN TECHNOLOGIES, INC. reassignment AXSUN TECHNOLOGIES, INC. RELEASE OF FIRST LIEN SECURITY INTEREST IN INTELLECTUAL PROPERTY Assignors: JPMORGAN CHASE BANK, N.A., AS COLLATERAL AGENT
Assigned to AXSUN TECHNOLOGIES, INC. reassignment AXSUN TECHNOLOGIES, INC. RELEASE OF SECOND LIEN SECURITY INTEREST IN INTELLECTUAL PROPERTY Assignors: ROYAL BANK OF CANADA, AS COLLATERAL AGENT
Assigned to GOLUB CAPITAL MARKETS LLC, AS COLLATERAL AGENT reassignment GOLUB CAPITAL MARKETS LLC, AS COLLATERAL AGENT SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: Excelitas Technologies Corp.
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/10Arrangements of light sources specially adapted for spectrometry or colorimetry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • G01J3/42Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G01J3/433Modulation spectrometry; Derivative spectrometry
    • G01J3/4338Frequency modulated spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12Generating the spectrum; Monochromators
    • G01J3/26Generating the spectrum; Monochromators using multiple reflection, e.g. Fabry-Perot interferometer, variable interference filters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • G01N2021/396Type of laser source
    • G01N2021/399Diode laser
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/05Flow-through cuvettes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis

Definitions

  • BTU Blunt Thermal Unit
  • energy-content monitors are used to analyze the BTU content of natural gas at producing wells and transfer points, and also at the points of consumption.
  • NIR near infrared
  • GC gas chromatographs
  • the hydrocarbons present in the natural gas are separated based on the retention time on a heated column.
  • the BTU or energy content is calculated by summing up the concentration of the different hydrocarbon species and applying published mathematical equations.
  • NIR based analysis operates on a different principle.
  • a spectrum of the sample is collected. Light at different wavelengths is absorbed based on the concentration of functional groups, such as C—H, C ⁇ C—H, C ⁇ C—H, N—H, and O—H, present in the molecules of the gas.
  • the spectrum of the natural gas is a sum of the different species present such as methane, ethane, isobutene, n-butane, propane, etc.
  • Mathematical models based on chemometrics derive a relationship between the spectra and the concentration of the property of interest, such as BTU or energy content.
  • the resulting calibration model is applied to each spectrum from the gas, and the BTU content can be reported to a local control or data logging system.
  • the invention features a system of gas property monitoring. It comprises a gas cell for containing a gas of interest and a semiconductor tunable laser spectroscopy system for generating a tunable signal that is transmitted through the gas of interest in the gas cell and detecting the tunable signal after transmission through the gas of interest.
  • An analyzer is provided for relating a spectral response of the gas of interest to a property of interest, such as an energy content of the gas of interest.
  • a pressure sensor for determining a pressure of the gas of interest and a temperature sensor for determining a temperature of the gas of interest are further provided.
  • the analyzer may use the pressure and the temperature to normalize the spectra before chemometric analysis is used to determine the property of interest.
  • a hydrogen concentration sensor is provided. This sensor is used to detect the presence and amount of hydrogen in the gas of interest to address the situation where the narrow spectral signatures of the hydrogen are not able to be accurately detected by the broader spectral linewidth of the tunable laser.
  • FIG. 1 is a schematic diagram showing a BTU or energy-content monitoring system according to an embodiment of the invention
  • FIG. 2 is block diagram of the spectroscopy system of the monitoring system according to an embodiment of the invention.
  • FIG. 3 illustrates an external cavity laser used in the spectroscopy system of one embodiment
  • FIG. 4 is a plot showing the spectral response of exemplary natural gas components.
  • FIG. 1 shows a system configuration for a BTU or energy-content monitoring system 10 , which has been constructed according to the principles of the present.
  • the system 10 comprises a spectroscopy system 100 , enclosed in an explosion proof enclosure 12 .
  • the spectroscopy system 100 further comprises a wireless data interface 11 , supporting an 802.11b communications interface for control of the spectroscopy system and for uploading of spectroscopic data from the system 100 to an analyzer computer 101 .
  • the spectroscopy measurements are taken in a gas cell 14 .
  • the cell 14 is designed to operate in the wavelength range from 1550-1800 nanometers (nm) at ambient temperatures (0 to +50° C.) and pressures up to 600 pounds per square inch (psi). Under normal operating conditions, the cell 14 will be at ambient ( ⁇ 60° C.) temperature and 100 psi.
  • Two stainless steel-clad fiber optic cables 16 , 18 connect the spectroscopy system 100 to the gas cell 14 .
  • the configuration is suitable for monitoring of natural gas.
  • a tunable laser signal from the spectroscopy system 100 is transmitted to the gas cell 14 in output cable 16 .
  • the tunable laser signal then propagates through the gas atmosphere in the gas cell 14 .
  • the laser signal is then collected into the input cable 18 for transmission to the spectroscopic system detector 100 .
  • the light output from the spectroscopy system 100 on the output fiber 16 which is single mode optical fiber with polarization control such as polarization maintaining or other polarization controlling fiber.
  • a sample probe/tap 20 is installed into the gas line 22 . This extracts a representative sample of gas and transports it to a sample conditioning system 24 .
  • the sample conditioning system 24 removes water and any condensate present, using a filter 26 . It also controls the pressure and flow to/through the gas cell using a first flow/pressure control valve 28 and a second flow/pressure control valve 36 .
  • a pressure sensor 30 and a temperature sensor 32 are also installed in-line with the sample cell 14 .
  • the pressure and temperature sensors 30 , 32 are read by the analyzer 101 and logged to enable compensation of the spectroscopy data based on a pressure and temperature.
  • a hydrogen concentration sensor 33 is provided in line with the pressure and temperature sensors 30 , 32 .
  • This hydrogen sensor is used to detect the presence and amount of hydrogen gas, diatomic hydrogen, in the gas of interest to address the situation where the narrow spectral signatures of the hydrogen are not able to be accurately detected by the broader spectral linewidth of the tunable laser of the spectroscopy system 100 .
  • the gas of interest continuously flows through the flow cell 14 and is scanned and analyzed. After exiting the gas cell, the gas can be returned to a low pressure point 42 .
  • a valve or restrictor 40 is used to create a pressure gradient between a high pressure region 38 , where the gas sample is drawn from, and the low pressure region 42 where the gas is returned to the pipe 22 .
  • the sampled gas is flared.
  • the analyzer 101 contains mathematical models based on chemometrics that relate the spectral data from the spectroscopy system 100 , the temperature data from temperature sensor 32 , hydrogen concentration from the hydrogen detector 33 , and pressure data from pressure 30 to the concentration of the property of interest, such as BTU or energy content.
  • the resulting calibration model is applied to each spectrum generated by the spectroscopy system 100 from the gas in the gas cell 14 , and the BTU concentration is reported to a local control or data logging system.
  • FIG. 2 shows the spectroscopy system 100 according to one embodiment. This system is discussed in more detail in U.S. patent application Ser. No. 11/419,993, filed May 23, 2006, by Flanders, et al., which is incorporated herein by this reference in its entirety.
  • two tunable semiconductor sources 50 - 1 and 50 - 2 are provided to generate tunable signals in different, adjacent spectral bands to increase spectral range. In a current embodiment, only a single source is used that emits in the range from 1550 to 1800 nm.
  • the tunable sources 50 - 1 , 50 - 2 have corresponding semiconductor chips 230 that are paired with microelectromechanical (MEMS) Fabry Perot tunable filters 200 to create external cavity tunable lasers (ECL).
  • MEMS microelectromechanical
  • Each of semiconductor sources 230 and tunable filters 200 of the tunable sources 50 - 1 , 50 - 2 are controlled by a system controller 60 .
  • a digital signal processor core 61 drives the sources and tunable filters via separate digital to analog converters D/A 140 , 142 .
  • Respective single mode optical fibers 52 - 1 and 52 - 2 carry the tunable signals from each of the sources 50 - 1 , 50 - 2 .
  • a wavelength amplitude referencing system 102 combines the tunable signals from each of the sources 50 - 1 , 50 - 2 onto the output fiber 16 while also performing amplitude and wavelength detection.
  • a polarizing beam combiner 110 is used to combine the tunable signals for each of the sources.
  • a wavelength reference tap 105 directs a portion of the combined beam to a quartz reference etalon 111 and a wavelength reference detector 112 .
  • An amplitude reference tap 116 directs a portion of the combined beam to an amplitude reference detector 114 .
  • Each of these detectors 112 , 114 is monitored by the system controller 60 via separate analog to digital converters 62 , 64 .
  • the tunable filters 200 are continuously scanned over the spectral scan band.
  • the tunable signal is transmitted to the gas sample of interest in gas cell 14 via the output optical fiber 16 .
  • the tunable signal from the sample is then collected on the input fiber and transmitted to a signal detector 70 , connected to the input fiber 18 , is then digitized by the detector's analog to digital converter 66 .
  • the typical measurement time is less than 2 seconds (with signal averaging).
  • the digital to analog converter 66 samples the detector 70 to provide a resolution of greater than 3.5 cm ⁇ 1 .
  • every point of every scan is referenced.
  • the signal from the wavelength reference detector 112 is a fringe pattern, analogous to the He-Ne reference signal in an FT-IR. This provides real-time wavelength referencing.
  • An optical bench 104 on which the reference system 102 is implemented is thermostat-controlled, ensuring both short- and long-term dimensional stability for the etalon 110 , and thus both short- and long-term wavelength reproducibility.
  • FIG. 3 illustrates an embodiment of the tunable ECL's in the tunable sources 50 - 1 , 50 - 2 .
  • This ECL system is discussed in more detail in U.S. patent application Ser. No. 11/158,617, filed Jun. 22, 2005, by Flanders, et al., which is incorporated herein by this reference in its entirety.
  • a reflective SOA 230 is used.
  • a first mirror of the laser cavity 236 is a facet 234 of the SOA gain chip 230 that has a highly reflecting (HR) coating 232 .
  • the other mirror of the laser cavity 236 is provided by an angled MEMS Fabry-Perot tunable filter 200 comprising an opposed curved mirror 212 and a flat mirror 210 .
  • An intracavity lens 238 is used to collimate or collect the light from an AR coated facet 240 of the SOA 230 and generally form a beam waist 242 to launch the light into the resonant filter 200 and then couple light from the filter 200 back into the chip 230 .
  • the light output from the laser cavity 236 is provided to the output fiber 16 , which is single mode fiber with polarization control such as polarization maintaining or other polarization controlling fiber.
  • FIG. 4 shows the spectral responses of some representative components of natural gas and other hydrocarbons. As illustrated, the CH range, from 1550 to 1800 nm provides unique signatures for the components, while having relatively low water absorption.

Landscapes

  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

A system of gas property monitoring comprises a gas cell for containing a gas of interest and a semiconductor tunable laser spectroscopy system for generating a tunable signal that is transmitted through the gas of interest in the gas cell and detecting the tunable signal after transmission through the gas of interest. An analyzer is provided for relating a spectral response of the gas of interest to a property of interest, such as an energy content of the gas of interest.

Description

RELATED APPLICATIONS
This application claims the benefit under 35 USC 119(e) of Provisional Application Nos. 60/752,303, filed on Dec. 20, 2005 and 60/775,465, filed Feb. 21, 2006, both of which are incorporated herein by this reference in their entirety.
BACKGROUND OF THE INVENTION
BTU (British Thermal Unit) or energy-content monitors are used to analyze the BTU content of natural gas at producing wells and transfer points, and also at the points of consumption. Previous work has showed the possibility of accurately performing this analysis by near infrared (NIR) spectroscopy, but commercially available instrumentation was too complex and expensive to be deployed widely. Instead gas chromatographs (GC) are currently used widely to perform this BTU monitoring. Nonetheless, there are several advantages to using NIR for this analysis including lower total cost of ownership, lower maintenance, faster response (seconds instead of minutes or tens of minutes), and the NIR approach requires no consumables such as carrier and fuel gases required by the GC.
In a GC analysis, the hydrocarbons present in the natural gas are separated based on the retention time on a heated column. The BTU or energy content is calculated by summing up the concentration of the different hydrocarbon species and applying published mathematical equations.
NIR based analysis operates on a different principle. A spectrum of the sample is collected. Light at different wavelengths is absorbed based on the concentration of functional groups, such as C—H, C═C—H, C═C—H, N—H, and O—H, present in the molecules of the gas. The spectrum of the natural gas is a sum of the different species present such as methane, ethane, isobutene, n-butane, propane, etc.
Mathematical models based on chemometrics derive a relationship between the spectra and the concentration of the property of interest, such as BTU or energy content. The resulting calibration model is applied to each spectrum from the gas, and the BTU content can be reported to a local control or data logging system.
SUMMARY OF THE INVENTION
In general according to one aspect, the invention features a system of gas property monitoring. It comprises a gas cell for containing a gas of interest and a semiconductor tunable laser spectroscopy system for generating a tunable signal that is transmitted through the gas of interest in the gas cell and detecting the tunable signal after transmission through the gas of interest. An analyzer is provided for relating a spectral response of the gas of interest to a property of interest, such as an energy content of the gas of interest.
In a preferred embodiment, a pressure sensor for determining a pressure of the gas of interest and a temperature sensor for determining a temperature of the gas of interest are further provided. The analyzer may use the pressure and the temperature to normalize the spectra before chemometric analysis is used to determine the property of interest. In a further modification, a hydrogen concentration sensor is provided. This sensor is used to detect the presence and amount of hydrogen in the gas of interest to address the situation where the narrow spectral signatures of the hydrogen are not able to be accurately detected by the broader spectral linewidth of the tunable laser.
The above and other features of the invention including various novel details of construction and combinations of parts, and other advantages, will now be more particularly described with reference to the accompanying drawings and pointed out in the claims. It will be understood that the particular method and device embodying the invention are shown by way of illustration and not as a limitation of the invention. The principles and features of this invention may be employed in various and numerous embodiments without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings, reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale; emphasis has instead been placed upon illustrating the principles of the invention. Of the drawings:
FIG. 1 is a schematic diagram showing a BTU or energy-content monitoring system according to an embodiment of the invention;
FIG. 2 is block diagram of the spectroscopy system of the monitoring system according to an embodiment of the invention;
FIG. 3 illustrates an external cavity laser used in the spectroscopy system of one embodiment; and
FIG. 4 is a plot showing the spectral response of exemplary natural gas components.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a system configuration for a BTU or energy-content monitoring system 10, which has been constructed according to the principles of the present.
The system 10 comprises a spectroscopy system 100, enclosed in an explosion proof enclosure 12. In one implementation, the spectroscopy system 100 further comprises a wireless data interface 11, supporting an 802.11b communications interface for control of the spectroscopy system and for uploading of spectroscopic data from the system 100 to an analyzer computer 101.
The spectroscopy measurements are taken in a gas cell 14. In one example, the cell 14 is designed to operate in the wavelength range from 1550-1800 nanometers (nm) at ambient temperatures (0 to +50° C.) and pressures up to 600 pounds per square inch (psi). Under normal operating conditions, the cell 14 will be at ambient (<60° C.) temperature and 100 psi.
Two stainless steel-clad fiber optic cables 16, 18 connect the spectroscopy system 100 to the gas cell 14. The configuration is suitable for monitoring of natural gas. Specifically, a tunable laser signal from the spectroscopy system 100 is transmitted to the gas cell 14 in output cable 16. The tunable laser signal then propagates through the gas atmosphere in the gas cell 14. The laser signal is then collected into the input cable 18 for transmission to the spectroscopic system detector 100. In this example, the light output from the spectroscopy system 100 on the output fiber 16, which is single mode optical fiber with polarization control such as polarization maintaining or other polarization controlling fiber.
A sample probe/tap 20 is installed into the gas line 22. This extracts a representative sample of gas and transports it to a sample conditioning system 24. The sample conditioning system 24 removes water and any condensate present, using a filter 26. It also controls the pressure and flow to/through the gas cell using a first flow/pressure control valve 28 and a second flow/pressure control valve 36.
A pressure sensor 30 and a temperature sensor 32 are also installed in-line with the sample cell 14. The pressure and temperature sensors 30, 32 are read by the analyzer 101 and logged to enable compensation of the spectroscopy data based on a pressure and temperature.
In a further embodiment, a hydrogen concentration sensor 33 is provided in line with the pressure and temperature sensors 30, 32. This hydrogen sensor is used to detect the presence and amount of hydrogen gas, diatomic hydrogen, in the gas of interest to address the situation where the narrow spectral signatures of the hydrogen are not able to be accurately detected by the broader spectral linewidth of the tunable laser of the spectroscopy system 100.
The gas of interest continuously flows through the flow cell 14 and is scanned and analyzed. After exiting the gas cell, the gas can be returned to a low pressure point 42. Specifically, a valve or restrictor 40 is used to create a pressure gradient between a high pressure region 38, where the gas sample is drawn from, and the low pressure region 42 where the gas is returned to the pipe 22. In another embodiment, the sampled gas is flared.
The analyzer 101 contains mathematical models based on chemometrics that relate the spectral data from the spectroscopy system 100, the temperature data from temperature sensor 32, hydrogen concentration from the hydrogen detector 33, and pressure data from pressure 30 to the concentration of the property of interest, such as BTU or energy content. The resulting calibration model is applied to each spectrum generated by the spectroscopy system 100 from the gas in the gas cell 14, and the BTU concentration is reported to a local control or data logging system.
FIG. 2 shows the spectroscopy system 100 according to one embodiment. This system is discussed in more detail in U.S. patent application Ser. No. 11/419,993, filed May 23, 2006, by Flanders, et al., which is incorporated herein by this reference in its entirety.
In one embodiment, two tunable semiconductor sources 50-1 and 50-2 are provided to generate tunable signals in different, adjacent spectral bands to increase spectral range. In a current embodiment, only a single source is used that emits in the range from 1550 to 1800 nm. The tunable sources 50-1, 50-2 have corresponding semiconductor chips 230 that are paired with microelectromechanical (MEMS) Fabry Perot tunable filters 200 to create external cavity tunable lasers (ECL).
Each of semiconductor sources 230 and tunable filters 200 of the tunable sources 50-1, 50-2 are controlled by a system controller 60. Specifically a digital signal processor core 61 drives the sources and tunable filters via separate digital to analog converters D/ A 140, 142.
Respective single mode optical fibers 52-1 and 52-2 carry the tunable signals from each of the sources 50-1, 50-2.
A wavelength amplitude referencing system 102 combines the tunable signals from each of the sources 50-1, 50-2 onto the output fiber 16 while also performing amplitude and wavelength detection.
In more detail, a polarizing beam combiner 110 is used to combine the tunable signals for each of the sources. A wavelength reference tap 105 directs a portion of the combined beam to a quartz reference etalon 111 and a wavelength reference detector 112. An amplitude reference tap 116 directs a portion of the combined beam to an amplitude reference detector 114. Each of these detectors 112, 114 is monitored by the system controller 60 via separate analog to digital converters 62, 64.
In operation, the tunable filters 200 are continuously scanned over the spectral scan band. The tunable signal is transmitted to the gas sample of interest in gas cell 14 via the output optical fiber 16. The tunable signal from the sample is then collected on the input fiber and transmitted to a signal detector 70, connected to the input fiber 18, is then digitized by the detector's analog to digital converter 66. In one embodiment, the typical measurement time is less than 2 seconds (with signal averaging). The digital to analog converter 66 samples the detector 70 to provide a resolution of greater than 3.5 cm−1.
In the preferred embodiment, every point of every scan is referenced. As the sources 50-1, 50-2 of the spectrometer scan, the signal from the wavelength reference detector 112 is a fringe pattern, analogous to the He-Ne reference signal in an FT-IR. This provides real-time wavelength referencing.
An optical bench 104 on which the reference system 102 is implemented is thermostat-controlled, ensuring both short- and long-term dimensional stability for the etalon 110, and thus both short- and long-term wavelength reproducibility.
FIG. 3 illustrates an embodiment of the tunable ECL's in the tunable sources 50-1, 50-2. This ECL system is discussed in more detail in U.S. patent application Ser. No. 11/158,617, filed Jun. 22, 2005, by Flanders, et al., which is incorporated herein by this reference in its entirety.
In a current embodiment, a reflective SOA 230 is used. As a result, a first mirror of the laser cavity 236 is a facet 234 of the SOA gain chip 230 that has a highly reflecting (HR) coating 232. The other mirror of the laser cavity 236 is provided by an angled MEMS Fabry-Perot tunable filter 200 comprising an opposed curved mirror 212 and a flat mirror 210. An intracavity lens 238 is used to collimate or collect the light from an AR coated facet 240 of the SOA 230 and generally form a beam waist 242 to launch the light into the resonant filter 200 and then couple light from the filter 200 back into the chip 230.
In this example, the light output from the laser cavity 236 is provided to the output fiber 16, which is single mode fiber with polarization control such as polarization maintaining or other polarization controlling fiber.
FIG. 4 shows the spectral responses of some representative components of natural gas and other hydrocarbons. As illustrated, the CH range, from 1550 to 1800 nm provides unique signatures for the components, while having relatively low water absorption.
While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.

Claims (17)

1. A system of gas property monitoring, comprising:
a gas cell for containing a gas of interest;
a semiconductor tunable laser spectroscopy system for generating a tunable signal that is transmitted through the gas of interest in the gas cell and detecting the tunable signal after transmission through the gas of interest to determine a spectral response of the gas of interest, wherein a spectral width of the tunable signal from the semiconductor tunable laser spectroscopy system is too broad to accurately detect a concentration of diatomic hydrogen due to associated narrow spectral lines of the diatomic hydrogen;
a hydrogen sensor for detecting a concentration of the diatomic hydrogen in the gas of interest, and
an analyzer for relating the spectral response of the gas of interest in combination with the detected concentration of the diatomic hydrogen to an energy content of the gas of interest, wherein the analyzer uses the detected concentration of diatomic hydrogen to compensate the energy content determined with respect to the spectral response of the gas of interest.
2. A system as claimed in claim 1, further comprising a pressure sensor for determining a pressure of the gas of interest, the analyzer further using the pressure to determine the energy content.
3. A system as claimed in claim 1, further comprising a temperature sensor for determining a temperature of the gas of interest, the analyzer further using the temperature to determine the energy content.
4. A system as claimed in claim 1, further comprising a pressure sensor for determining a pressure of the gas of interest and a temperature sensor for determining a temperature of the gas of interest, the analyzer further using the pressure and the temperature to determine the energy content.
5. A system as claimed in claim 1, further comprising an output optical fiber for transmitting the tunable signal to the gas cell.
6. A system as claimed in claim 1, further comprising an output optical fiber for transmitting the tunable signal to the gas cell, wherein the output optical fiber is single mode fiber.
7. A system as claimed in claim 1, further comprising an output optical fiber for transmitting the tunable signal to the gas cell, wherein the output optical fiber is polarization controlling fiber.
8. A method for monitoring a property of a gas of interest, comprising:
providing a sample of a gas;
generating a tunable signal with a semiconductor laser that is transmitted through the gas, wherein the step of generating the tunable signal comprises generating the tunable signal with a spectral width that is too broad to accurately detect a concentration of diatomic hydrogen due to associated narrow spectral lines of the diatomic hydrogen;
detecting the tunable signal after transmission through the gas to determine a spectral response of the gas;
detecting a concentration of the diatomic hydrogen in the gas of interest, and
relating the spectral response of the gas in combination with the detected concentration of the diatomic hydrogen to an energy content of the gas by using the detected concentration of diatomic hydrogen to compensate the energy content determined with respect to the spectral response of the gas.
9. A method as claimed in claim 8, further comprising:
determining a pressure of the gas; and
using the pressure to determine the energy content.
10. A method as claimed in claim 9, further comprising:
determining a temperature of the gas of interest; and
using the temperature to determine the energy content.
11. A system of gas property monitoring, comprising:
a gas cell for containing a gas of interest;
an external cavity semiconductor tunable laser spectroscopy system for generating a tunable signal that is transmitted through the gas of interest in the gas cell and detecting the tunable signal after transmission through the gas of interest to determine spectral response of gas of interest, the tunable laser comprising a semiconductor optical amplifier, a tunable filter, and a lens for coupling light between the semiconductor optical amplifier and the tunable filter;
an analyzer for relating the spectral response of the gas of interest to-an energy content of the gas; and
a hydrogen sensor for detecting a concentration of diatomic hydrogen in the gas of interest, and the analyzer relating a spectral response of the gas of interest and the detected concentration of the diatomic hydrogen of the energy content.
12. A system as claimed in claim 11, further comprising a pressure sensor for determining a pressure of the gas of interest, the analyzer further using the pressure to determine the energy content.
13. A system as claimed in claim 11, further comprising a temperature sensor for determining a temperature of the gas of interest, the analyzer further using the temperature to determine the energy content.
14. A system as claimed in claim 11, further comprising a pressure sensor for determining a pressure of the gas of interest and a temperature sensor for determining a temperature of the gas of interest, the analyzer further using the pressure and the temperature to determine the energy content.
15. A system as claimed in claim 11, further comprising an output optical fiber for transmitting the tunable signal to the gas cell.
16. A system as claimed in claim 11, further comprising an output optical fiber for transmitting the tunable signal to the gas cell, wherein the output optical fiber is single mode fiber.
17. A system as claimed in claim 11, further comprising an output optical fiber for transmitting the tunable signal to the gas cell, wherein the output optical fiber is polarization controlling fiber.
US11/613,291 2005-12-20 2006-12-20 Semiconductor laser natural gas analysis system and method Expired - Fee Related US7764379B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/613,291 US7764379B1 (en) 2005-12-20 2006-12-20 Semiconductor laser natural gas analysis system and method

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US75230305P 2005-12-20 2005-12-20
US77546506P 2006-02-21 2006-02-21
US11/613,291 US7764379B1 (en) 2005-12-20 2006-12-20 Semiconductor laser natural gas analysis system and method

Publications (1)

Publication Number Publication Date
US7764379B1 true US7764379B1 (en) 2010-07-27

Family

ID=42341900

Family Applications (1)

Application Number Title Priority Date Filing Date
US11/613,291 Expired - Fee Related US7764379B1 (en) 2005-12-20 2006-12-20 Semiconductor laser natural gas analysis system and method

Country Status (1)

Country Link
US (1) US7764379B1 (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013023426A1 (en) * 2011-08-18 2013-02-21 天津大学 Multiband aliased inner cavity gas sensing system and sensing method
US20130230271A1 (en) * 2012-03-05 2013-09-05 Pukyong National University Industry-University Cooperation Foundation Optical Fiber Hydrogen Sensor and Method of Measuring Hydrogen Concentration Using the Same
US20140326049A1 (en) * 2013-05-06 2014-11-06 Serguei Zelepouga Method and apparatus for real-time measurement of fuel gas compositions and heating values
US9869634B2 (en) 2014-08-27 2018-01-16 General Electric Company System and method for dissolved gas analysis
US10024768B1 (en) * 2016-06-17 2018-07-17 Markwest Energy Partners, L.P. System, method, and apparatus for determining air emissions during pig receiver depressurization
US10094781B2 (en) 2014-04-14 2018-10-09 General Electric Company Methods and systems to analyze a gas-mixture
US20220074850A1 (en) * 2020-09-04 2022-03-10 Carrier Corporation Gas detection system

Citations (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2286985A (en) * 1939-07-04 1942-06-16 Du Pont Analysis of gas mixtures
EP0822977A1 (en) 1995-04-20 1998-02-11 Diacrin, Inc. Modified cells and methods for inhibiting xenograft rejection
US5822058A (en) 1997-01-21 1998-10-13 Spectral Sciences, Inc. Systems and methods for optically measuring properties of hydrocarbon fuel gases
US6038023A (en) 1998-07-31 2000-03-14 The Research Foundation Of State University Of New York Sensors for detection and spectroscopy
US6072576A (en) 1996-12-31 2000-06-06 Exxon Chemical Patents Inc. On-line control of a chemical process plant
US6157455A (en) * 1997-06-06 2000-12-05 Gaz De France Method and apparatus for determining the calorific value of a natural gas optically and in real time
EP1070955A2 (en) 1999-07-21 2001-01-24 Zellweger Analytics Limited Measurement of gas calorific value with infrared radiation
US20010054900A1 (en) 2000-05-15 2001-12-27 Sadahiko Yokoyama Method and apparatus for identifying plastics
US6420695B1 (en) 1998-03-24 2002-07-16 Schlumberger Industries, S.A. Method for wavelength calibration of an electromagnetic radiation filtering device
EP1141677B1 (en) 1999-01-05 2002-07-31 Flowcomp Systemtechnik GmbH Method of determining the gas quality
US6536946B1 (en) 1998-03-24 2003-03-25 Schlumberger Industries, S.A. Device and method for directly measuring calorific energy contained in a fuel gas
US6539775B2 (en) 2001-02-13 2003-04-01 Wolfgang H. Driftmeier Method and apparatus for the measurement of the interchangeability of LPG/air mixtures with natural gas
US6552793B1 (en) 1999-10-14 2003-04-22 Flowcomp Systemtechnik Gmbh Determination of the quality of a gas
US6555820B1 (en) 1998-08-24 2003-04-29 Flow Comp Systemtechnik Gmbh Photometric device and photometric method for determining the gross calorific value of a test gas
US6559945B1 (en) 1998-08-07 2003-05-06 Schlumberger Resource Management Services, Inc. Method for measuring spectral absorption in a body and device therefor
US6590647B2 (en) 2001-05-04 2003-07-08 Schlumberger Technology Corporation Physical property determination using surface enhanced raman emissions
US20040120366A1 (en) * 2002-12-20 2004-06-24 Sean Chang Method of designing the cavity length of a tunable laser light source
US20060044562A1 (en) * 2004-08-25 2006-03-02 Norsk Elektro Optikk As Gas monitor
US7298490B2 (en) * 2005-09-30 2007-11-20 Los Gatos Research Hydrogen sensor based upon quadrupole absorption spectroscopy

Patent Citations (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2286985A (en) * 1939-07-04 1942-06-16 Du Pont Analysis of gas mixtures
EP0822977A1 (en) 1995-04-20 1998-02-11 Diacrin, Inc. Modified cells and methods for inhibiting xenograft rejection
US6072576A (en) 1996-12-31 2000-06-06 Exxon Chemical Patents Inc. On-line control of a chemical process plant
US5822058A (en) 1997-01-21 1998-10-13 Spectral Sciences, Inc. Systems and methods for optically measuring properties of hydrocarbon fuel gases
US6157455A (en) * 1997-06-06 2000-12-05 Gaz De France Method and apparatus for determining the calorific value of a natural gas optically and in real time
US6536946B1 (en) 1998-03-24 2003-03-25 Schlumberger Industries, S.A. Device and method for directly measuring calorific energy contained in a fuel gas
US6420695B1 (en) 1998-03-24 2002-07-16 Schlumberger Industries, S.A. Method for wavelength calibration of an electromagnetic radiation filtering device
US6038023A (en) 1998-07-31 2000-03-14 The Research Foundation Of State University Of New York Sensors for detection and spectroscopy
US6559945B1 (en) 1998-08-07 2003-05-06 Schlumberger Resource Management Services, Inc. Method for measuring spectral absorption in a body and device therefor
US6555820B1 (en) 1998-08-24 2003-04-29 Flow Comp Systemtechnik Gmbh Photometric device and photometric method for determining the gross calorific value of a test gas
US6941230B1 (en) 1999-01-05 2005-09-06 Flowcomp Systemtechnik Gmbh Method of determining the gas quality
EP1141677B1 (en) 1999-01-05 2002-07-31 Flowcomp Systemtechnik GmbH Method of determining the gas quality
EP1070955A2 (en) 1999-07-21 2001-01-24 Zellweger Analytics Limited Measurement of gas calorific value with infrared radiation
US6552793B1 (en) 1999-10-14 2003-04-22 Flowcomp Systemtechnik Gmbh Determination of the quality of a gas
US20010054900A1 (en) 2000-05-15 2001-12-27 Sadahiko Yokoyama Method and apparatus for identifying plastics
US6539775B2 (en) 2001-02-13 2003-04-01 Wolfgang H. Driftmeier Method and apparatus for the measurement of the interchangeability of LPG/air mixtures with natural gas
US6590647B2 (en) 2001-05-04 2003-07-08 Schlumberger Technology Corporation Physical property determination using surface enhanced raman emissions
US20040120366A1 (en) * 2002-12-20 2004-06-24 Sean Chang Method of designing the cavity length of a tunable laser light source
US20060044562A1 (en) * 2004-08-25 2006-03-02 Norsk Elektro Optikk As Gas monitor
US7298490B2 (en) * 2005-09-30 2007-11-20 Los Gatos Research Hydrogen sensor based upon quadrupole absorption spectroscopy

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Brown, Chris W. et al., "Feasibility of On-line Monitoring of the BTU Content of Natural Gas with a Near-Infrared Fiber Optic System," Applied Spectroscopy, vol. 47, No. 6, pp. 812-815, 1993.
Goldstein, N. et al., "Real-Time Optical BTU Measurement of Natural Gas at Line Pressure," 4th International Symposium on Fluid Flow Measurement, Denver, Colorado, 13 pages, Jun. 27-30, 1999.
Somesfalean, G. et al., "Temporal correlation scheme for spectroscopic gas analysis using multimode diode lasers," Applied Physics Letters 86, 184102, 3 pages, 2005.

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013023426A1 (en) * 2011-08-18 2013-02-21 天津大学 Multiband aliased inner cavity gas sensing system and sensing method
US8934100B2 (en) 2011-08-18 2015-01-13 Tianjin University Multi-band multiplexing intra-cavity gas sensing system and method
US20130230271A1 (en) * 2012-03-05 2013-09-05 Pukyong National University Industry-University Cooperation Foundation Optical Fiber Hydrogen Sensor and Method of Measuring Hydrogen Concentration Using the Same
US8842944B2 (en) * 2012-03-05 2014-09-23 Pukyong National University Industry-University Cooperation Foundation Optical fiber hydrogen sensor and method of measuring hydrogen concentration using the same
US20140326049A1 (en) * 2013-05-06 2014-11-06 Serguei Zelepouga Method and apparatus for real-time measurement of fuel gas compositions and heating values
US9291610B2 (en) * 2013-05-06 2016-03-22 Gas Technology Institute Method and apparatus for real-time measurement of fuel gas compositions and heating values
US10094781B2 (en) 2014-04-14 2018-10-09 General Electric Company Methods and systems to analyze a gas-mixture
US10495578B2 (en) 2014-04-14 2019-12-03 General Electric Company Methods and systems to analyze a gas-mixture
US9869634B2 (en) 2014-08-27 2018-01-16 General Electric Company System and method for dissolved gas analysis
US10024768B1 (en) * 2016-06-17 2018-07-17 Markwest Energy Partners, L.P. System, method, and apparatus for determining air emissions during pig receiver depressurization
US20220074850A1 (en) * 2020-09-04 2022-03-10 Carrier Corporation Gas detection system

Similar Documents

Publication Publication Date Title
Chen et al. Highly sensitive photoacoustic multi-gas analyzer combined with mid-infrared broadband source and near-infrared laser
CA3085305C (en) Hydrogen gas sensor and method for measurement of hydrogen under ambient and elevated pressure
Hodgkinson et al. Optical gas sensing: a review
US7764379B1 (en) Semiconductor laser natural gas analysis system and method
Zhou et al. Development of a fast temperature sensor for combustion gases using a single tunable diode laser
US7781737B2 (en) Apparatus and methods for oil-water-gas analysis using terahertz radiation
US9097583B2 (en) Long-path infrared spectrometer
Engelbrecht A compact NIR fiber-optic diode laser spectrometer for CO and CO2:: analysis of observed 2f wavelength modulation spectroscopy line shapes
US20060044562A1 (en) Gas monitor
Weibring et al. Ultra-high-precision mid-IR spectrometer II: system description and spectroscopic performance
Ruxton et al. Tunable diode laser spectroscopy with wavelength modulation: Elimination of residual amplitude modulation in a phasor decomposition approach
Willer et al. Fiber-optic evanescent-field laser sensor for in-situ gas diagnostics
EP2895828A1 (en) Method and system for determining energy content and detecting contaminants in a fluid stream
Edwards et al. A diode laser based gas monitor suitable for measurement of trace gas exchange using micrometeorological techniques
Lambrecht et al. Broadband spectroscopy with external cavity quantum cascade lasers beyond conventional absorption measurements
CN114945816A (en) Stimulated Raman spectrometer for real-time, high resolution molecular analysis of gases in hollow core optical fiber
CN112748087A (en) Multi-component detection device and method based on temperature tuning absorption spectrum technology
US20030132389A1 (en) Method for monitoring and controlling the high temperature reducing combustion atmosphere
US7064329B2 (en) Amplifier-enhanced optical analysis system and method
Kühnreich et al. Direct single-mode fibre-coupled miniature White cell for laser absorption spectroscopy
US20030038237A1 (en) Amplifier-enhanced optical analysis system and method
CN114397271A (en) Detection device and method for spectral analysis of greenhouse gases
Cai et al. A sensor for measurements of temperature and water concentration using a single tunable diode laser near 1.4 μm
CA2870177A1 (en) High resolution calibration-free infrared spectrometer
Mitra Mid-infrared spectroscopy and challenges in industrial environment

Legal Events

Date Code Title Description
AS Assignment

Owner name: AXSUN TECHNOLOGIES, INC., MASSACHUSETTS

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:MCDERMOTT, LAWRENCE;REEL/FRAME:018998/0022

Effective date: 20070309

STCF Information on status: patent grant

Free format text: PATENTED CASE

FPAY Fee payment

Year of fee payment: 4

FEPP Fee payment procedure

Free format text: PAT HOLDER CLAIMS SMALL ENTITY STATUS, ENTITY STATUS SET TO SMALL (ORIGINAL EVENT CODE: LTOS); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

AS Assignment

Owner name: AXSUN TECHNOLOGIES LLC, MASSACHUSETTS

Free format text: CHANGE OF NAME;ASSIGNOR:AXSUN TECHNOLOGIES, INC.;REEL/FRAME:037901/0152

Effective date: 20151015

AS Assignment

Owner name: AXSUN TECHNOLOGIES, INC., MASSACHUSETTS

Free format text: CHANGE OF NAME;ASSIGNOR:AXSUN TECHNOLOGIES, LLC;REEL/FRAME:043733/0195

Effective date: 20160329

MAFP Maintenance fee payment

Free format text: PAYMENT OF MAINTENANCE FEE, 8TH YR, SMALL ENTITY (ORIGINAL EVENT CODE: M2552)

Year of fee payment: 8

AS Assignment

Owner name: ROYAL BANK OF CANADA, AS COLLATERAL AGENT, NEW YORK

Free format text: SECOND LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT;ASSIGNOR:AXSUN TECHNOLOGIES, INC.;REEL/FRAME:048000/0711

Effective date: 20190102

Owner name: ROYAL BANK OF CANADA, AS COLLATERAL AGENT, NEW YOR

Free format text: SECOND LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT;ASSIGNOR:AXSUN TECHNOLOGIES, INC.;REEL/FRAME:048000/0711

Effective date: 20190102

Owner name: JPMORGAN CHASE BANK, N.A., NEW YORK

Free format text: FIRST LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT;ASSIGNOR:AXSUN TECHNOLOGIES, INC.;REEL/FRAME:048000/0692

Effective date: 20190102

FEPP Fee payment procedure

Free format text: ENTITY STATUS SET TO UNDISCOUNTED (ORIGINAL EVENT CODE: BIG.); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

AS Assignment

Owner name: EXCELITAS TECHNOLOGIES CORP., MASSACHUSETTS

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:AXSUN TECHNOLOGIES INC.;REEL/FRAME:054698/0911

Effective date: 20201210

FEPP Fee payment procedure

Free format text: MAINTENANCE FEE REMINDER MAILED (ORIGINAL EVENT CODE: REM.); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

AS Assignment

Owner name: GOLUB CAPITAL MARKETS LLC, AS COLLATERAL AGENT, ILLINOIS

Free format text: SECURITY INTEREST;ASSIGNOR:EXCELITAS TECHNOLOGIES CORP.;REEL/FRAME:061164/0582

Effective date: 20220812

Owner name: AXSUN TECHNOLOGIES, INC., MASSACHUSETTS

Free format text: RELEASE OF SECOND LIEN SECURITY INTEREST IN INTELLECTUAL PROPERTY;ASSIGNOR:ROYAL BANK OF CANADA, AS COLLATERAL AGENT;REEL/FRAME:061161/0942

Effective date: 20220811

Owner name: AXSUN TECHNOLOGIES, INC., MASSACHUSETTS

Free format text: RELEASE OF FIRST LIEN SECURITY INTEREST IN INTELLECTUAL PROPERTY;ASSIGNOR:JPMORGAN CHASE BANK, N.A., AS COLLATERAL AGENT;REEL/FRAME:061161/0854

Effective date: 20220811

LAPS Lapse for failure to pay maintenance fees

Free format text: PATENT EXPIRED FOR FAILURE TO PAY MAINTENANCE FEES (ORIGINAL EVENT CODE: EXP.); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

STCH Information on status: patent discontinuation

Free format text: PATENT EXPIRED DUE TO NONPAYMENT OF MAINTENANCE FEES UNDER 37 CFR 1.362

FP Lapsed due to failure to pay maintenance fee

Effective date: 20220727